Laboratory of Chromatography, Institute of Chemistry at Sao Carlos, University of Sao Paulo, P.O Box 780, Sao Carlos 13566590, Brazil.
Laboratory of Chromatography, Institute of Chemistry at Sao Carlos, University of Sao Paulo, P.O Box 780, Sao Carlos 13566590, Brazil.
J Chromatogr A. 2022 Dec 6;1685:463618. doi: 10.1016/j.chroma.2022.463618. Epub 2022 Oct 29.
Graphene and graphene-derived substances are cutting-edge materials receiving increasing attention in the analytical chemistry field. Graphene oxide sheets bonded to amino silica particles functionalized with octadecyl (C18) groups and endcapped, also known as SiGO-C18ec, have been successfully employed as extraction phases and in analytical columns associated with conventional liquid chromatography (LC). In this work, SiGO-C18ec particles of 3, 5, and 10 µm nominal id were employed to pack capillary LC columns (100 mm long x 0.3 mm id), and their performance in the gradient mode was evaluated and compared. A 3 µm C18 capillary LC column (50 x 0.3 mm) was used as a reference column. Eight analytes having different polarities and topological surface areas were selected as a probe in this study: carbofuran clomazone, hexazinone, carbamazepine, citalopram, clomipramine, desipramine, and ochratoxin A. Studies about orthogonality were performed to investigate the orthogonality between the SiGO-C18ec and C18 phases. Among the SiGO-C18ec phases investigated, the column packed with 5 µm SiGO-C18ec particles presented the best peak capacity (29) in 15 min. Additionally, the performance of the columns packed with 5 µm SiGO-C18ec particles overcame the performance of the C18 columns used. Significant orthogonality was found between C18 and SiGO-C18ec packed columns; however, no significant differences were found between columns packed with SiGO-C18ec particles of different diameters.
石墨烯和石墨烯衍生物质是分析化学领域中受到越来越多关注的前沿材料。氧化石墨烯片与十八烷基(C18)官能化的氨基硅粒子结合并端基封端,也称为 SiGO-C18ec,已成功用作萃取相和与常规液相色谱(LC)相关的分析柱。在这项工作中,使用了 3、5 和 10 µm 名义 id 的 SiGO-C18ec 颗粒来填充毛细管 LC 柱(100 mm 长 x 0.3 mm id),并评估和比较了它们在梯度模式下的性能。使用 3 µm C18 毛细管 LC 柱(50 x 0.3 mm)作为参考柱。本研究选择了 8 种具有不同极性和拓扑表面积的分析物作为探针:克百威、氯唑酮、己酮、西酞普兰、氯米帕明、去甲丙咪嗪和赭曲霉毒素 A。进行了正交性研究,以研究 SiGO-C18ec 和 C18 相之间的正交性。在所研究的 SiGO-C18ec 相中,填充有 5 µm SiGO-C18ec 颗粒的柱在 15 分钟内呈现出最佳的峰容量(29)。此外,填充有 5 µm SiGO-C18ec 颗粒的柱的性能优于使用的 C18 柱。在填充 C18 和 SiGO-C18ec 的柱子之间发现了显著的正交性;然而,在填充不同直径的 SiGO-C18ec 颗粒的柱子之间没有发现显著差异。